CN102309533A - Preparation method of total flavones of artemisia anomalas - Google Patents
Preparation method of total flavones of artemisia anomalas Download PDFInfo
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- CN102309533A CN102309533A CN201110187502A CN201110187502A CN102309533A CN 102309533 A CN102309533 A CN 102309533A CN 201110187502 A CN201110187502 A CN 201110187502A CN 201110187502 A CN201110187502 A CN 201110187502A CN 102309533 A CN102309533 A CN 102309533A
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- extraction
- total flavones
- artemisia anomalas
- ethanol
- artemisia
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Abstract
The invention discloses a preparation method of total flavones of artemisia anomalas, belonging to an extractivetechnique of total flavones, comprising the following steps: crushing dry artemisia anomalas, using the supper critical carbon dioxide fluid extraction technology and ethanol as carrying agent to obtain the extract, absorbing the extract with macroporous resin, carrying out elution with ethanol, carrying out concentration under reduced pressure, and carrying out freeze drying to obtain a product of total flavones of artemisia anomalas. The method has the advantages of simple and rapid operation without toxicity, and is a green production method.
Description
Technical field
The invention belongs to Separation of Natural Products purification field, relate to the preparation technology of active substance in the natural product, specifically is a kind of method for preparing of artemisia anomalas total flavones.
Background technology
Compositae mugwort artemisia anomalas
Artemisia anomalaS. Moore is with wounded in the battle all herbal medicine.Has clearing away summer-heat and eliminating dampness, blood circulation promoting competent silt, the effect of inducing menstruation to relieve menalgia.Be used for heatstroke, headache, enteritis, dysentery, amenorrhea stomachache, rheumatalgia, traumatic injury; Wound hemorrhage is controlled in external, mastitis.Artemisia anomalas contains flavonoid, Coumarins, sesquiterpene lactones and organic acid.The artemisia anomalas general flavone content is about 6%.
At present, there be long, shortcoming, domestic related patent U.S. Patent No. of not seeing artemisia anomalas total flavones method for preparing as yet such as the solvent use amount is big of extraction time in the relevant method of extracting arteanoflavone.
Summary of the invention
The method for preparing that the purpose of this invention is to provide a kind of artemisia anomalas total flavones, promptly a kind of method of utilizing supercritical carbon dioxide extraction and macroporous resin to prepare the artemisia anomalas total flavones.
For realizing above-mentioned purpose, the present invention adopts following technical scheme: exsiccant artemisia anomalas is pulverized, put into extractor; And carry agent with ethanol, and carry the 25-30% of agent consumption for the extraction inventory, the extraction kettle temperature is 35-42 ℃; The extraction-container temperature is 30-40 ℃; Extraction kettle pressure is 28-35MPa, and extraction-container pressure is 6-6.5MPa, CO
2Flow is 25-38L/h, and the extraction time is 2-3h, resolves the extract that obtains and adds aqueous dispersion; Obtain the sample solution of 0.8-1.2mg/ml, adopt the macroporous resin dynamic adsorption, after absorption is accomplished; Elder generation's water flush away water-solubility impurity; The ethanol of reuse 60-70% carries out eluting, the eluent concentrating under reduced pressure, and lyophilization promptly gets artemisia anomalas total flavones product.
The optional AB-8 of described macroporous resin, S-8, ADS-7 or HPD-300 type, ethanol are 65% ethanol.
The present invention has the following advantages:
1, the present invention adopts the supercritical carbon dioxide extraction technology, and not only the leaching process time spent lacks, and solvent load is few, and equipment automatization is easy and simple to handle, has improved economic benefit and social benefit.
2, adopt the inventive method to prepare the artemisia anomalas total flavones, its total flavones rate of transform is greater than 80%, in the products obtained therefrom general flavone content more than 55%, and favorable reproducibility, resin can reuse.
3, process stabilizing of the present invention, product purity is high.
Below in conjunction with specific embodiment the present invention is done further explanation, but do not limit the present invention in any way.
The specific embodiment
Embodiment 1
Exsiccant artemisia anomalas is pulverized, got 2kg, put into extractor, and carry agent with ethanol, carry the agent consumption and be 25% of extraction inventory, it is 42 ℃ that the extraction kettle temperature is set, and the extraction-container temperature is 40 ℃, and extraction kettle pressure is 28MPa, CO
2Flow is 30L/h, behind the extraction 2h, parses extract; Extraction-container pressure is 6MPa, and extract adds aqueous dispersion, obtains the sample solution of 0.8mg/ml; Adopt AB-8 type macroporous resin dynamic adsorption, after absorption is accomplished, wash the solubility impurity that anhydrates with 8L earlier; The ethanol of reuse 65% carries out eluting, the eluent concentrating under reduced pressure, and lyophilization promptly gets artemisia anomalas total flavones product 56g.
Embodiment 2
Exsiccant artemisia anomalas is pulverized, got 2kg, put into extractor, and carry agent with ethanol, carry the agent consumption and be 30% of extraction inventory, it is 38 ℃ that the extraction kettle temperature is set, and the extraction-container temperature is 35 ℃, and extraction kettle pressure is 30MPa, CO
2Flow is 25L/h, behind the extraction 2.5h, parses extract; Extraction-container pressure is 6.5MPa, and extract adds aqueous dispersion, obtains the sample solution of 1.2mg/ml; Adopt S-8 type macroporous resin dynamic adsorption, after absorption is accomplished, wash the solubility impurity that anhydrates with 10L earlier; The ethanol of reuse 65% carries out eluting, the eluent concentrating under reduced pressure, and lyophilization promptly gets artemisia anomalas total flavones product 52g.
Embodiment 3
Exsiccant artemisia anomalas is pulverized, got 2kg, put into extractor, and carry agent with ethanol, carry the agent consumption and be 25% of extraction inventory, it is 35 ℃ that the extraction kettle temperature is set, and the extraction-container temperature is 30 ℃, and extraction kettle pressure is 35MPa, CO
2Flow is 38L/h, behind the extraction 3h, parses extract; Extraction-container pressure is 6MPa, and extract adds aqueous dispersion, obtains the sample solution of 1mg/ml; Adopt ADS-7 type macroporous resin dynamic adsorption, after absorption is accomplished, wash the solubility impurity that anhydrates with 8L earlier; The ethanol of reuse 60% carries out eluting, the eluent concentrating under reduced pressure, and lyophilization promptly gets artemisia anomalas total flavones product 63g.
Embodiment 4
Exsiccant artemisia anomalas is pulverized, got 5kg, put into extractor, and carry agent with ethanol, carry the agent consumption and be 25% of extraction inventory, it is 35 ℃ that the extraction kettle temperature is set, and the extraction-container temperature is 30 ℃, and extraction kettle pressure is 30MPa, CO
2Flow is 28L/h, behind the extraction 2h, parses extract; Extraction-container pressure is 6.5MPa, and extract is scattered in the water, obtains the sample solution of 1.2mg/ml; Adopt AB-8 type macroporous resin dynamic adsorption, after absorption is accomplished, wash the solubility impurity that anhydrates with 18L earlier; The ethanol of reuse 70% carries out eluting, the eluent concentrating under reduced pressure, and lyophilization promptly gets artemisia anomalas total flavones product 151g.
Embodiment 5
Exsiccant artemisia anomalas is pulverized, got 5kg, put into extractor, and carry agent with ethanol, carry the agent consumption and be 30% of extraction inventory, it is 40 ℃ that the extraction kettle temperature is set, and the extraction-container temperature is 40 ℃, and extraction kettle pressure is 35MPa, CO
2Flow is 38L/h, behind the extraction 2h, parses extract; Extraction-container pressure is 6.5MPa, and extract adds aqueous dispersion, obtains the sample solution of 1mg/ml; Adopt HPD-300 type macroporous resin dynamic adsorption, after absorption is accomplished, wash the solubility impurity that anhydrates with 18L earlier; The ethanol of reuse 70% carries out eluting, the eluent concentrating under reduced pressure, and lyophilization promptly gets artemisia anomalas total flavones product 170g.
Claims (3)
1. the method for preparing of an artemisia anomalas total flavones is characterized in that exsiccant artemisia anomalas is pulverized, and adopts supercritical CO
2The fluid extraction method, and carry agent with ethanol, resolve the extract that obtains and be scattered in the water, adopt macroporous resin, dynamic adsorption, after absorption is accomplished, ethanol elution, concentrating under reduced pressure, lyophilization promptly gets artemisia anomalas total flavones product.
2. the method for preparing of a kind of artemisia anomalas total flavones as claimed in claim 1 is characterized in that: described supercritical CO
2The fluid extraction condition: the extraction kettle temperature is 35-42 ℃, and the extraction-container temperature is 30-40 ℃, and extraction kettle pressure is 28-35MPa, and extraction-container pressure is 6-6.5MPa, CO
2Flow is 25-38L/h, carries the 25-30% of agent consumption for the extraction inventory, and the extraction time is 2-3h.
3. the method for preparing of a kind of artemisia anomalas total flavones as claimed in claim 1 is characterized in that: the optional AB-8 of described macroporous resin, S-8, ADS-7 or HPD-300 type, ethanol are 65% ethanol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110187502A CN102309533A (en) | 2011-07-06 | 2011-07-06 | Preparation method of total flavones of artemisia anomalas |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110187502A CN102309533A (en) | 2011-07-06 | 2011-07-06 | Preparation method of total flavones of artemisia anomalas |
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| CN102309533A true CN102309533A (en) | 2012-01-11 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
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| CN201110187502A Pending CN102309533A (en) | 2011-07-06 | 2011-07-06 | Preparation method of total flavones of artemisia anomalas |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105646194A (en) * | 2014-11-21 | 2016-06-08 | 中国人民解放军第二军医大学 | Preparation and application of artemisia anomala s.moore extract 3,4-dihydroxycinnamic acid |
| CN105732558A (en) * | 2014-12-12 | 2016-07-06 | 中国人民解放军第二军医大学 | Extraction method of monomer arteanoflavone from Artemisia plants, and application of the arteanoflavone in preparation of medicine for inhibiting staphylococcus aureus |
-
2011
- 2011-07-06 CN CN201110187502A patent/CN102309533A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105646194A (en) * | 2014-11-21 | 2016-06-08 | 中国人民解放军第二军医大学 | Preparation and application of artemisia anomala s.moore extract 3,4-dihydroxycinnamic acid |
| CN105646194B (en) * | 2014-11-21 | 2018-05-15 | 中国人民解放军第二军医大学 | The preparation and application of artemisia anomalas extract 3,4- dihydroxycinnamic acids |
| CN105732558A (en) * | 2014-12-12 | 2016-07-06 | 中国人民解放军第二军医大学 | Extraction method of monomer arteanoflavone from Artemisia plants, and application of the arteanoflavone in preparation of medicine for inhibiting staphylococcus aureus |
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Application publication date: 20120111 |